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AbstractLocal corn produce starch with high whiteness, but has not been developed in the Pharmaceutical Industry. Starch is one of the raw materials that are used as an excipient of tablet. This study aimed to obtain corn starch as an excipient meets the standards and determine the effect of concentration sodium metabisulfite and drying time on the quality of starch. The research method using a completely randomized design with two factors, the concentration of sodium metabisulfite (3000 ppm, 2500 ppm and 2000 ppm) and drying time (24 hours, 28 hours). Starch was isolated by the wet method and starch were analyzed qualitatively, tested physicochemical properties, and is characterized by instrument Fourier Transform Infrared (FTIR) and scanning electron microscope (SEM). Results of the analysis showed that the starch from the corn meet the standards as pharmaceutical excipients. Concentration Sodium metabisulfite has very significant effect on yield, moisture content, and sulfite residue while drying time significantly affect yield, moisture content, compressibility and sulfite residues. combined treatment of drying time and the concentration of sodium metabisulfite has significant effect on yield, pH and compressibility. 28-hour drying time and concentration of 2500 ppm Sodium metabisulfite give the best effect on the quality of corn starch. Index TermsCorn Starch, drying time, local corn, sodium metabisulphite, excipients. I. INTRODUCTION Based on the data from the Ministry of Health, it is found that 95% of raw materials of drugs in Indonesia are still dependent on imports [1]. Dependence on imported raw materials makes Indonesia a nation that is less self-sufficient in terms of raw materials, while Indonesia has abundant biodiversity and has great potential as a producer of raw material for medicine [2]. Starch is a raw material widely used in the food industry and pharmaceutical industry, namely as an excipient in pharmaceutical preparations such as fillers, binders, disintegrator tablets [3]. Starch is widely used in the pharmaceutical industry because it is inert, inexpensive, and white [4]. Corn is a plant producing starch with starch content of about 54.1 to 71.7% [5]. Corn is composed of various types of amylose and amylopectin starch in the form of low-to-high [6]. High content of amylopectin can be found in the Local Corn Manuscript received April 17, 2015; revised June 20, 2015. The authors are with the Pharmacy Faculty, Universitas Padjadjaran, Indonesia (e-mail: [email protected]). Pulut. Local corn is white maize contained in several regions in Indonesia [7]. The advantages of local corn white are the color of corn and fairly high amylopectin content [8]. According to the Ohio State University extension in corn starch amylopectin content is glutinous almost 100% [9]. In the process of corn starch isolation, soaking in sodium metabisulphite takes more than 20 hours at a temperature of 48 - 52 o C [10]. According to Slamet, immersion in a solution of sodium metabisulfite can prevent browning reaction on starch made so that the resulting product will produce a brighter color. In addition, the sodium sulfite ion content metabisufit also damage the matrix proteins play a role in the endosperm of corn with a way of breaking the disulfide bonds of proteins that can facilitate the release of starch in the endosperm of corn [10]. Another stage in the isolation of starch is drying. The drying process to reduce the moisture content of the material and prevents spoilage microorganisms or materials due to enzymatic processes [11] which can affect the quality of the resulting starch. This study was conducted to develop the use of local corn in Industrial raw materials and to determine the effect of immersion concentration Sodium metabisulfite and drying time on the quality and physicochemical properties of corn starch produced Indonesian local corn. II. PROCEDURE A. Corn Starch Isolation Isolation of corn starch corn was finely done by cleaning the skin and hair of corn. Shell corn soaked with a solution of sodium metabisulfite concentration of 2000 ppm, 2500 ppm and 3000 ppm for 24 hours at a temperature of 50° C. Shell corn subsequently rinsed with distilled water (1: 2) and drained. then finely milled corn grinding machine with the addition of distilled water (1: 3) to form slurry, finely ground with the addition of distilled water (1: 2) using a blender, the slurry were filtered using gauze and distilled water added about 1.5 liter accompanied by stirring so that separate between the left over corn flesh and starch suspension. Corn starch suspension was precipitated for 24 hours at room temperature. The precipitate formed is separated from the filtrate and included in the chamber which already contains distilled water. This deposition process was repeated twice each for 2 hours. Last precipitation process, added a solution Optimization of Starch from Indonesian Local Corn with Concentration Variation of Sodium Metabisuphite and Drying Time Richie A. I. Chandra, Sriwidodo, Aliya Nur Hasanah, and Rahma Agustina International Journal of Chemical Engineering and Applications, Vol. 7, No. 2, April 2016 89 DOI: 10.7763/IJCEA.2016.V7.549
Transcript

Abstract—Local corn produce starch with high whiteness,

but has not been developed in the Pharmaceutical Industry.

Starch is one of the raw materials that are used as an excipient

of tablet. This study aimed to obtain corn starch as an excipient

meets the standards and determine the effect of concentration

sodium metabisulfite and drying time on the quality of starch.

The research method using a completely randomized design

with two factors, the concentration of sodium metabisulfite

(3000 ppm, 2500 ppm and 2000 ppm) and drying time (24 hours,

28 hours). Starch was isolated by the wet method and starch

were analyzed qualitatively, tested physicochemical properties,

and is characterized by instrument Fourier Transform Infrared

(FTIR) and scanning electron microscope (SEM). Results of the

analysis showed that the starch from the corn meet the

standards as pharmaceutical excipients. Concentration Sodium

metabisulfite has very significant effect on yield, moisture

content, and sulfite residue while drying time significantly affect

yield, moisture content, compressibility and sulfite residues.

combined treatment of drying time and the concentration of

sodium metabisulfite has significant effect on yield, pH and

compressibility. 28-hour drying time and concentration of 2500

ppm Sodium metabisulfite give the best effect on the quality of

corn starch.

Index Terms—Corn Starch, drying time, local corn, sodium

metabisulphite, excipients.

I. INTRODUCTION

Based on the data from the Ministry of Health, it is found

that 95% of raw materials of drugs in Indonesia are still

dependent on imports [1]. Dependence on imported raw

materials makes Indonesia a nation that is less self-sufficient

in terms of raw materials, while Indonesia has abundant

biodiversity and has great potential as a producer of raw

material for medicine [2].

Starch is a raw material widely used in the food industry

and pharmaceutical industry, namely as an excipient in

pharmaceutical preparations such as fillers, binders,

disintegrator tablets [3]. Starch is widely used in the

pharmaceutical industry because it is inert, inexpensive, and

white [4].

Corn is a plant producing starch with starch content of

about 54.1 to 71.7% [5]. Corn is composed of various types of

amylose and amylopectin starch in the form of low-to-high [6].

High content of amylopectin can be found in the Local Corn

Manuscript received April 17, 2015; revised June 20, 2015.

The authors are with the Pharmacy Faculty, Universitas Padjadjaran,

Indonesia (e-mail: [email protected]).

Pulut.

Local corn is white maize contained in several regions in

Indonesia [7]. The advantages of local corn white are the

color of corn and fairly high amylopectin content [8].

According to the Ohio State University extension in corn

starch amylopectin content is glutinous almost 100% [9].

In the process of corn starch isolation, soaking in sodium

metabisulphite takes more than 20 hours at a temperature of

48 - 52 oC [10]. According to Slamet, immersion in a solution

of sodium metabisulfite can prevent browning reaction on

starch made so that the resulting product will produce a

brighter color. In addition, the sodium sulfite ion content

metabisufit also damage the matrix proteins play a role in the

endosperm of corn with a way of breaking the disulfide bonds

of proteins that can facilitate the release of starch in the

endosperm of corn [10].

Another stage in the isolation of starch is drying. The

drying process to reduce the moisture content of the material

and prevents spoilage microorganisms or materials due to

enzymatic processes [11] which can affect the quality of the

resulting starch.

This study was conducted to develop the use of local corn

in Industrial raw materials and to determine the effect of

immersion concentration Sodium metabisulfite and drying

time on the quality and physicochemical properties of corn

starch produced Indonesian local corn.

II. PROCEDURE

A. Corn Starch Isolation

Isolation of corn starch corn was finely done by cleaning

the skin and hair of corn. Shell corn soaked with a solution of

sodium metabisulfite concentration of 2000 ppm, 2500 ppm

and 3000 ppm for 24 hours at a temperature of 50° C. Shell

corn subsequently rinsed with distilled water (1: 2) and

drained. then finely milled corn grinding machine with the

addition of distilled water (1: 3) to form slurry, finely ground

with the addition of distilled water (1: 2) using a blender, the

slurry were filtered using gauze and distilled water added

about 1.5 liter accompanied by stirring so that separate

between the left over corn flesh and starch suspension. Corn

starch suspension was precipitated for 24 hours at room

temperature. The precipitate formed is separated from the

filtrate and included in the chamber which already contains

distilled water. This deposition process was repeated twice

each for 2 hours. Last precipitation process, added a solution

Optimization of Starch from Indonesian Local Corn with

Concentration Variation of Sodium Metabisuphite and

Drying Time

Richie A. I. Chandra, Sriwidodo, Aliya Nur Hasanah, and Rahma Agustina

International Journal of Chemical Engineering and Applications, Vol. 7, No. 2, April 2016

89DOI: 10.7763/IJCEA.2016.V7.549

of 0.1 N NaOH and precipitated (± 3 hours). The filtrate was

then separated from the grains of starch and starch is washed

with water to remove residual NaOH, the washing process

was repeated 5 times until pH starch neutral. The precipitate

was separated from the filtrate, to then dried in an oven at 50°

C with drying time (24 hours and 28 hours). Starch crushed

and sieved using a 80 and no.100 mesh sieve. Calculated %

yield of starch produced.

B. Quality Controll and Physico Chemical Properties of

Corn Starch

To get the corn starch which meets the requirements as

pharmaceutical excipients, required characterization of the

maize starch include: Organoleptic, solubility, Microscopy,

qualitative test with iodine, Losses drying, pH [12],

Smoothness [13], SO2 residue levels [14], compressibility

[15], specific gravity [16], microbial contamination [13], the

degree of white [17], Heavy Metal Contamination [13] and

corn starch characterization instrument method is by using

Fourier Transform Infrared [18] and Scanning Electron

Microscope [19]. Complete study randomized design with

two factors that the results were compared with the

requirements contained in literatur. Experiment was done

with two replications of samples. The data were analyzed by

Two Way ANOVA with significance level α = 0.01.

III. RESULT AND DISCUSSION

A. Result of Isolation

The results showed that the concentration of sodium

metabisulfite soaking with 3000 ppm resulted in the highest %

yield (see Table I) compared to the concentration of sodium

metabisulphite 2500 ppm and 2000 ppm. The higher

concentration of sodium metabisulfite then yield to the higher

corn starch. This is because the dissolution of sodium

metabisulfite in water resulting in the formation of Na+ ion

and bisulfite ion (HSO3-), bisulfite ion reacts with H

+ to form

SO2. The use of SO2 is very important because of SO2 as a

reducing agent capable of breaking the disulfide bonds that

wraps matrix protein starch granules, so as to free the starch

granules. Additionally SO2 able to create favorable conditions

for the growth of lactic acid bacteria (Lactobacillus). The

lactic acid produced by lactic acid bacteria can help the

separation of starch and increase the amount of starch

produced. Lactic acid can increase the softening seed,

endosperm proteins dissolve and weaken the endosperm cell

walls [20].

The yield of starch with a 24-hour drying time has starch

yield greater than 28 hours drying time (see Table II). It is

because the water content is evaporated more. This is

consistent with the statement Desrosier where the longer the

drying time the water content is evaporated more and more so

that the weight of the material to be reduced and the resulting

starch yield will be lower [21]. There is interaction between

the concentration of sodium metabisulfite with drying time.

Where the higher concentration of sodium metabisulfite and

the shorter length of time drying the% yield of starch

produced will increase.

B. Qualitative analysis of Corn Starch

1) Organoleptic

From the organoleptic examination at six samples tested

showed results in accordance with the standards in the

USP-NF XXX XXV white starch, in the form of a fine

powder has no odor and has no taste (see Table III). From the

test results it can be concluded that the starch obtained from

each different treatment has met the criteria required

organoleptic in the USP-NF XXX XXV [12].

2) Solubility

From the testing that has been made known that the

solubility of local corn starch at a concentration sticky

Sodium metabisulfite and different drying time obtained

starch solubility in water and ethanol 95% is not soluble (see

Table III). This is consistent with the solubility properties of

starch which is expressed in the United States

Pharmacopeia-National Formulary XXX XXV [12].

Insolubility of corn starch is closely related to the

carbohydrate content of corn starch, which generally contains

20% amylose and 80% amylopectin, which is known

amylopectin insoluble in water.

3) Results analysis of corn starch iodine test

Identification of corn starch with sodium metabisulfite and

the concentration of different drying is done by suspending

the starch with water that is heated to form starch solution that

viscous. Starch formed complex with iodine reagent that

changes color to blue. This is caused by the molecular

structure of the starch in the form of a spiral that will traped

the iodine molecule and forming a blue color. When starch is

heated, the spiral will be stretchable, iodine molecules apart

so that the blue color disappears [22]. From the experimental

results obtained from the 6 samples tested starch to form a

blue color complex after the addition of iodine (see Table III).

4) Microscopic

The results of the microscopic appearance of the local corn

starch at a concentration of sodium metabisulfite and different

drying time showed no significant differences too, each

sample shows the characteristic cross-sectional picture of

corn starch as in the United States Pharmacopeia-National

Formulary XXX XXV which are hillus in the middle, in the

form of a real cavity or crevice numbered 2 through 5, no

lamella, and under visible light irradiation with a black cross

shape cut at the hilum

C. The Results of the Examination of the Physicochemical

Properties of Corn Starch

1) Loss of drying

Based on testing of 6 samples of starch with different

treatment - found that all six different starch sample drying

shrinkage still meet the requirements specified in the USP-NF

XXX XXV ≤ 15%. The results showed concentrations of

sodium metabisulfite soaking 3000 ppm resulted % higher

drying shrinkage (see Table IV) compared with the

concentration of sodium metabislufit 2500 ppm and 2000

ppm. The greater concentration of sodium metabisulphite, the

greater the drying shrinkage. This is not in line with the

research conducted by Prabasini et al. (2013) which states

that the greater the concentration of sodium metabisulphite

International Journal of Chemical Engineering and Applications, Vol. 7, No. 2, April 2016

90

then drying shrinkage is getting smaller due to the destruction

of tissue by sulfite compounds which can speed up the drying

process [23].

This may be due to differences in the amount of starch

suspension produced in each treatment. In the treatment of

sodium metabisulphite concentration of 3000 ppm amount of

starch suspension produced more while the area of drying and

drying temperature is used as the starch concentration of 2500

ppm and 2000 ppm, it causes drying shrinkage by treatment

with sodium metabisulphite 3000 ppm much larger.

Drying shrinkage with a 24-hour drying time has a drying

shrinkage greater than 28 hours drying time (see Table V) this

is consistent with Desrosier statement stating that the longer

drying and higher drying temperatures cause the water content

in the material so much evaporate the water content and the

weight of the material is reduced. Interaction Na2S2O5

concentration and drying time did not have a significant

influence on the drying shrinkage.

2) Sulfite residue

Of the six samples of starch with different treatment, it was

found that all six samples of starch still meet the requirements

of sulfite residues listed in the USP-NF XXX XXV ≤ 50 ppm.

The result showed Na2S2O5 concentration of 3000 ppm

soaking produce sulfite residual values are higher (table 4)

compared with Na2S2O5 concentration of 2500 ppm and 2000

ppm. SO2 residual value increases with increase in the

concentration of sodium metabisulfite this is due to the higher

concentration of sodium metabisulfite is used, the more

sulfites which binds to the aldehyde or ketone on reducing

sugar and form a hydroxy compound sulfonate [24].

At the 24 hours drying time has sulfite residual values

smaller than 28 hours drying time (see Table V). The longer

the drying time, the higher the value of sulfite residues is

consistent with the research Farida (2007) which states that

the higher the temperature and the longer drying the moisture

content of the material will be lower so that residual sulfite

total is higher [25]. Interaction between Sodium metabisulfite

concentration and drying time is not very significant effect on

residual sulfite. Total absorption of sulphite in a material is

influenced by several factors, including the size of the

material, the use of SO2 concentration, temperature and time

sulfuring, temperature and state during the drying process

[26].

3) Microbial contamination

Total Plate Count

Total plate count is a method to determine the number of

bacteria in a sample. These tests are known to regulate the

development of many bacteria samples, where the total

bacterial dependent formation of bacteria in a growth medium

and each resulting bacterial colony forming a single [27]. As

for the number of colonies of bacteria present in the tested

sample still qualify contained in NFPA 01-3727-1995 ie

anaerobic bacteria for corn starch is smaller than! 0 6 CFU/

gram.

Based on the test results showed that sodium metabisulfite

and drying time is not very significant effect on the number of

bacterial colonies. Highest number of colonies obtained at

treatment concentrations of sodium metabisulphite 2000 ppm

and 28 hours drying time.

The difference in the number of colonies of bacteria in the

sample may be caused by other factors such as lack of aseptic

conditions or the processing of samples and sample storage is

not good so the samples contaminated by bacteria originating

either from the surrounding air and water used during the

production process.

Fungus Yeast

Figures mold/yeast showed a contamination of mold / yeast

in the preparation being examined. Each dosage requires

numeric limit mold/yeast are still considered safe particular.

The calculation is performed for the number of 40-50 colonies.

Figures molds/yeasts expressed as the number of colonies of

mold/yeasts result multiplied by the dilution factor calculation.

As for the number of colonies of bacteria present in the tested

sample still qualify contained in NFPA 01-3727-1995 ie mold

colony for corn starch is less than 104 CFU / unit.

The results of the experiment showed that the concentration

of sodium metabisulfite and drying time did not have a

significant influence on the number of mold colonies. The

highest number of colonies bacteria obtained at treatment

concentrations of sodium metabisulphite 2000 ppm and 24

hours drying time.

The difference in the number of fungal colonies in the

sample may be caused by other factors such as lack of aseptic

conditions or the processing of samples and sample storage is

not good so contaminated by mold samples derived from

either ambient air or work tools used.

4) pH

The results showed immersion Na2S2O5 concentration

2000 ppm resulted in higher pH (see Table IV) compared with

Na2S2O5 concentration of 2500 ppm and 3000 ppm. this can

be caused by several other factors came into effect in addition

to the concentration of sodium metabisulfite ie NaOH with

distilled water washing process is less than perfect so there are

still many who are trapped in NaOH which causes the starch

starch to slightly alkaline pH, the process of mixing and starch

deposition during the isolation process less precise.

The pH value affects the optimum gel formation. Optimum

starch gel formation occurs at pH 4-7. Where high pH can

cause changes in the functional properties of corn starch,

which is more rapid gel formation, but its viscosity is reached

sooner down and when the heating was continued viscosity

will go down again. At pH 4-7 gel formation slower pace than

pH 10, but when the heating is continued, the viscosity does

not change [22].

Drying time did not have a significant influence on the pH

(see Table V) Where the pH value on a 24-hour drying time of

6.7 and the drying time of 28 hours the pH value of

6,6.Interaksi Na2S2O5 concentration and drying time has no

influence significantly on pH.

5) Fineness

The results showed all six samples still meet the

requirements of the fineness based SNI 01-3727-1995 ie

passes > 70% with a 80 degree mesh fineness of starch at a

concentration of sodium metabisulphite 3000 ppm and 2000

ppm have the highest degree of fineness is lower than the

concentration of 2500 ppm (see Table IV). based on that

result, it can be presumed degrees of fineness is not only

influenced by the concentration of Na2S2O5 but rather

International Journal of Chemical Engineering and Applications, Vol. 7, No. 2, April 2016

91

influenced by several other factors came into effect in

addition to the concentration of sodium metabisulfite one of

which is influenced by the process of manufacture of starch

that is in the process of milling and sieving the starch samples

were less than perfect. Subtlety is closely related to grain size

and determined to sift the powder with a sieve standar.Degree

subtlety showed the powder particle size uniformity which

would affect the homogenous distribution of the drug

compound, the size of the particles and granules associated

with the problem of compaction and tablet weight uniformity

[28].

While the drying time is based on data obtained no

significant effect on the degree of fineness (see Table V).

There is no significant influence of the interaction drying time

and the concentration of sodium metabisulfite to the degree of

fineness.

6) Compressability

Based on the result showed that the value of the

compressibility of samples from each treatment is still not

eligible listed in the Handbook of Pharmaceitical excipients

Fifth Edition is less than 30%. The results showed

compressibility starch at a concentration of sodium

metabisulphite 3000 ppm and 2000 ppm have compressibility

values higher than 2500 ppm (see Table IV) it can be due to

several other factors that take effect in addition to the

concentration of sodium metabisulfite one of which is the

distribution of grain size and shape partikel. The particle size

is getting smaller and more delicate, the greater cohesiveness

between particles, thereby increasing the value of the

compressibility.

While the effect of drying time on the compressibility was

found that the compressibility at 24 hours drying time is

greater than the drying time of 28 hours (see Table V). The

longer the drying time, the lower the water content. High

water levels will make the bonds between the particles

become stronger because of extensive contact between the

surface of the powder riding. If the attractive force between

powder particles is getting stronger, the powder will be more

compact and even higher the compresibility.

7) Thickness

The results showed that the concentration of Na2S2O5

immersion (see Table IV) and drying time (see Table V) have

no significant effect on the gravity of the resulting starch.

From the results of experiments that have been carried out the

true density of the results obtained in each treatment nearing

density value types are listed in the Handbook of

Pharmaceutical excipients Fifth Edition is 1,478 g / cm3. The

weight of a substance is influenced by several other factors

including the temperature, the volume of the substance, and

the substance period measured viscosity of the substance.

8) The degree of white

Tests carried out on samples of white degree of starch with

the best yield is the concentration of 3000 ppm Sodium

metabisulfite with 24-hour drying time and standard corn

starch (redwood). Color powder that will be used as an

excipient in accordance with the requirements must be white

in order not to affect the appearance of the resulting

preparation [29]. Therefore, it was necessary to measure to

measure the whiteness of the white color of the two samples.

Testing is done by using a Hunter Reflectometer. Where the

principle of tests performed by measuring the intensity of

light reflected by the surface of the test sample with a

wavelength of 457 nm using an appropriate filter and diffuse

lighting equipment and observations have perpendicular. The

whiteness of the test results of samples prepared starch has a

value of whiteness 78.27% ± 0.07 while the standard white

starch has a value of 79.65 ± 0.04 degrees. Based on ISO

standard no special requirements for the minimum value of

the degree of white corn starch, but the higher the percent

degree of white starch, the better and more attractive physical

appearance. The degree of starch as an excipient white sample

plays an important role because of the color produced

excipient can affect the color and physical appearance of the

preparation prepared as in tablet dosage. From the

measurement results seem values whiteness samples made has

approached the value whiteness of standard starch (redwood)

in the market.

9) Heavy metal contamination

Testing with AAS method was conducted to determine

heavy metal contamination of lead (Pb), Cadmium (Cd),

Copper (Cu), iron (Fe), mercury (Hg) and arsenic (As) of

local sticky corn starch. From the results of experiments that

have been carried out on samples of starch to yield the best

that starch samples with a concentration of 3000 ppm Sodium

metabisulfite and drying time 24 jam.didapatkan that the

heavy metal content in the samples still meet the requirements

specified in NFPA 01-3727 -, 1995 (see Table VI) From

Table 6 it can be seen that the value of the metal content of

iron (Fe) has not met the requirements of the USP-NF XXX

XXV. This could be because the content of the soil of each

planting areas generally contain metals minerals in a certain

amount, and there is also the possibility of the metal content

of lead, copper, cadmium, mercury, arsenic and iron in small

quantities [30]. In addition contamination can also occur from

a tool used for the isolation of starch such as grinding machine

which may be carried in the process of iron starch isolation.

Metal contamination is very important, because of the metal

exceeds the specified threshold can affect the health of the

human body such as the nervous system and respiratory.

D. Characterization of Corn Starch with Instrument

Method

1) Fourier transform infrared (FTIR)

Analysis of functional groups on the local sticky corn

starch powder with the best yield and standard corn starch

(redwood) was performed using instrument Fourier

Transform Infrared (FTIR). The resulting spectrum of process

analysis using FTIR instrument can be seen in Figure 1. The

infrared spectrum of a standard corn starch (Redwood)

indicates the main absorption at wave number 3375.9 cm -1

and 1644.7 cm-1. Peaks at a wavelength of 3375.9 cm-1

indicates the group hidroxil and wavelength 1644.7 cm-1

indicates the group C - H stretching. In the wave number of

860.9 cm-1 showed the presence of CH oop group band.

On local corn starch sticky with the best yield indicates the

main absorption at wave number 3337.3 cm -1 and 1644.2

cm-1. Spectrum peaks at a wavelength of 3337.3 cm-1

International Journal of Chemical Engineering and Applications, Vol. 7, No. 2, April 2016

92

indicates the group hidroxil and wavelength 1644.2 cm-1

indicates the group C - H stretching. In the wave number of

1147.9 cm-1 showed the presence of group C - O stretch, at

860.1 wave numbers show an oop group CH band

Based on the observations it can be concluded that the

infrared spectrum of local sticky corn starch when compared

with standard corn starch (redwood) gives similar spectrum

and point out the similarity of functional groups.

2) Scanning Electron Microscope (SEM)

Observation by SEM performed at 2500x magnification to

determine the general picture of the corn starch particles.

SEM results can be seen in Fig. 2.

TABLE I: EFFECT OF CONCENTRATION SODIUM METABISULFITE

AGAINST %YIELD

Concentraion Na2S2O5 % yield

3000 ppm 43,53a

2500 ppm 37,26b

2000 ppm 29,94c

Note: The figure shows followed by the same letter are not

significantly different at the level of α = 0.1

TABLE II: EFFECT OF DRYING TIME AGAINST %YIELD

Drying time % yield

24 hour 39,58a

28 hour 34,23b

Note: The figure shows followed by the same letter are not

significantly different at the level of

TABLE III: QUALITATIVE TESTING RESULTS STARCH SAMPLES

Test 3000ppm (24

hour)

3000ppm (28

hour)

2500ppm (24

hour)

2500ppm (28

hour)

2000ppm

(24 hour)

2000ppm (28

hour)

Colour White White White White White White

Taste Tasteless Tasteless Tasteless Tasteless Tasteless Tasteless

Smell Odorless Odorless Odorless Odorless Odorless Odorless

Solubility Insoluble Insoluble Insoluble Insoluble Insoluble Insoluble

Test with

Iodium

Positive Positive Positive Positive Positive Positive

TABLE IV: THE INFLUENCE OF THE CONCENTRATION OF SODIUM METABISULPHITE ON PHYSICOCHEMICAL PROPERTIES

Concentration

Na2S2O5

drying

shrinkage (%)

sulfite

residues

(%)

colonies of

bacteria

( ALT)

mold

colonies

( AKK)

pH fineness (%) Compresability

(%)

Weight

Type

3000 ppm 11,58a 4,7a 2,68x105 0 6,6b 99,6b 31,6a 1,36a

2500 ppm 11,43a 4,4b 2,55x105 16,67 6,3c 99,8a 29,1b 1,25a

2000 ppm 10,21b 4,0c 20,98x105 83,3 7,1a 99,5b 31,3a 1,2 1a

Note: The figure shows followed by the same letter are not significantly different at the level of α = 0.1

TABLE V: EFFECT OF DRYING TIME ON PHYSICOCHEMICAL PROPERTIES

drying time drying

shrinkage (%)

sulfite

residues

(%)

colonies of

bacteria

( ALT)

mold

colonies

( AKK)

pH fineness (%) Compresability

(%)

Weight

Type

24 hour 11,72a 3,84b 9,03x105 63,88 6,7a 99,7a 32,08a 1,38a

28 hour 10,43b 5,01a 8,45x105 2,77 6,6a 99,6a 29,33b 1,17a

Note: The figure shows followed by the same letter are not significantly different at the level of α = 0

TABLE VI: HEAVY METAL CONTAMINATION OF TEST RESULTS ON SAMPLES OF STARCH

type Metal total ( ppm) Requirements ( ppm)

Pb < 0,040 1 ( SNI 01-3727-1995)

Cu 0,18 10 ( SNI 01-3727-1995)

Cd 0,005 40 ( SNI 01-3727-1995)

As < 0,003 0,5 ( SNI 01-3727-1995)

Fe 21,3 10 (USP XXX-NF XXV)

Hg 0,005 0,05 ( SNI 01-3727-1995)

4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0

0.02

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

7.0

7.5

8.0

8.66

cm-1

%T

3375.9

1644.7

860.9

582.9

(a)

International Journal of Chemical Engineering and Applications, Vol. 7, No. 2, April 2016

93

= 0.1α

4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0

0.00

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

7.0

7.5

8.0

8.5

9.0

9.66

cm-1

%T

3337.31644.2 1147.9

860.1

585.3

471.6

(b)

Fig. 1. The results of the test with FTIR (a) standard corn starch (redwood); (b) sample R1L1 starch (sodium metabisulphite 3000 ppm and 24 hours

drying time).

Fig. 2. Results of SEM (a) Samples of starch in the best yield (b) standard starch (redwood)

From the observation with SEM, it appears that the

particles of corn starch and corn starch sticky standard

(redwood) are round, angled responsibility and tetragonal. At

the local corn starch sample standard sticky and showed

agglomeration fairly evenly. In addition, many individuals

either corn starch sample and standard plate-shaped arch with

large spaces. The shape of the curved plate with large spaces

and uneven particle surface even somewhat rough cause

starch has a pretty good porosity. However there are certain

individuals either on local corn starch samples sticky and

disability standards such as thinning, fractures and broken

individual starch this can be due to initial treatment during

theprocess of isolation of starch as the starch particle size

reduction stage with grinding tool which causes the starch

granules formed less than perfect and can also be caused by

the heating process is too long or at too high a temperature

that causes the starch granules and broken.

IV. CONCLUSIONS

Based on the research that has been conducted, FTIR and

SEM showed that the characteristics of corn starch obtained

from local sticky rice starch meets the standards as

pharmaceutical excipients as listed in the USP-NF XXX XXV,

SNI 01-3727-1995 and Handbook of Pharmaceitical

excipients Fifth Edition.

Based on research that has been done can be seen that the

concentration of sodium metabisulphite was highly

significant (α = 0.01) to the yield, drying shrinkage, and high

residual concentrations of sodium metabisulfite sulfit. The

value of yield higher, moisture content and residual sulfite

will be even greater. concentration of sodium metabisulphite

no significant effect on weight and type of microbial

contamination. Drying time was highly significant (α = 0.01)

to the yield, moisture content, residual sulfite and

compressibility. The longer the drying time, the lower the

value of the yield, moisture content and compressibility but

may increase the value of residual sulfite. Drying time has no

significant effect on specific gravity, pH, fineness and

microbial contamination. The interaction between the

concentration of sodium metabisulphite and drying time

significantly affect yield, pH and compressibility. The higher

concentration of sodium metabisulphite and old drying, the

lower value of the yield, pH and compressibility.

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Richie A. I. Chandra was born in Indoesia on 15th

August, 1984. He graduated from Pharmacy Bachelor

Program, Universitas Padjadjaran, Bandung, Indonesia,

2007 and Pharmacy Master Program from Universitas

Gadjah Mada, Yogyakarta, Indonesia, 2009

He is currently working as a lecturer in Departement

of Pharmaceutical Faculty Pharmacy Universitas

Padjadjaran. His research interests are pharmaceutical

technology, biotechnology and nanotechnology. He is a

member of Cosmetic Societies Scientist Indonesia.

Sriwidodo was born in Indoesia on 30th March, 1974.

He graduated from Pharmacy Bachelor Program,

Universitas Padjadjaran, Bandung, Indonesia, in 1997

and Pharmacy Master Program from Universitas

Padjajdaran, Bandung, Indonesia in 2007

He is currently working as a lecturer in the

Departement of of Pharmaceutical Faculty Pharmacy

Universitas Padjadjaran. His research interests are

pharmaceutical, and biotechnology.

Rahma Agustina was born in Tangerang on 26th August, 1992. She is a

student in Bachelor Program, Pharmacy Faculty, Universitas Padjadjaran,

Indonesia.

International Journal of Chemical Engineering and Applications, Vol. 7, No. 2, April 2016

95

Aliya Nur Hasanah was born in Indoesia on 12th

February, 1979. She graduated from Pharmacy Master

Program from Institute Technology Bandung,

Bandung, Indonesia in 2007. She is currently working

as a lecturer in the Departement of of

Pharmacochemistry Faculty Pharmacy Universitas

Padjadjaran. Her research interests are molecular

imprinting and separation method.


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